CN108303300A - Full-automatic liquid-liquid sample treatment instrument - Google Patents
Full-automatic liquid-liquid sample treatment instrument Download PDFInfo
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- CN108303300A CN108303300A CN201810144685.5A CN201810144685A CN108303300A CN 108303300 A CN108303300 A CN 108303300A CN 201810144685 A CN201810144685 A CN 201810144685A CN 108303300 A CN108303300 A CN 108303300A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0419—Solvent extraction of solutions which are liquid in combination with an electric or magnetic field or with vibrations
- B01D11/0423—Applying ultrasound
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0484—Controlling means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0488—Flow sheets
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N2035/00465—Separating and mixing arrangements
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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Abstract
The present invention relates to a kind of sample pre-treatments processing instruments, and in particular to a kind of Full Automatic Liquid liquid sample treatment instrument, the processing instrument include：Including：Solvent delivery system, piece-rate system, purification and concentration systems, control system, the solvent delivery system is made of solution feeding system and syringe pump system, it is attached respectively by main line between the solution feeding system, syringe pump system, purification and concentration systems, piece-rate system, the control system is electrically connected with solution feeding system, syringe pump system, purification and concentration systems, piece-rate system respectively；It is an advantage of the invention that：Fast, easy, not only time saving, laborsaving but also the error come due to different personnel operation and the multiple transition zone of sample can be reduced, while can be to avoid using a large amount of organic solvents to reduce the pollution to environment.
Description
Technical field
The present invention relates to a kind of sample pre-treatments processing instruments, and in particular to a kind of full-automatic liquid-liquid sample treatment instrument.
Background technology
The preceding processing of sample is important link, the purpose of sample pre-treatments in analytical chemistry：(1) the quilt of trace is concentrated
Part is surveyed, sensitivity is improved, reduces detection limit；(2) basic body and the other chaff interferents in sample are removed；By derivatization with
Other reactions make measured matter be converted into the high substance of detection sensitivity；Reduce sample quality and volume, be readily transported with
It preserves.
Since analysis sample composition is complicated, when detection, often interferes with each other, while the concentration of measured object is lower and lower, stablizes
Property come after a series of difficulties, the especially sampling of various Environmental and biological samples directly with change in time and space, thus to analysis measuring band
The possibility very little analyzed will could generally measure after sample pre-treatments.The analytic process of one intact sample
Substantially be divided into four steps, (1) sample collection, (2) sample pre-treatments, (3) analysis measure, (4) Data Management Analysis report as a result, tool
Statistics shows that they account for whole analysis time ratios and are respectively：Sample collection account for 6%, sample pre-treatments account for 61%, analysis measures 6%,
Data processing goes out report 27% so that pre-treatment occupies a large amount of detection time.
Sample-pretreating method has liquid night extraction, soxhlet extraction, chromatographic isolation, distillation, absorption, centrifugation, filtering etc. tens
Kind.There is the pretreatment technology of solid, liquid and gaseous sample from technique classification；Wherein, fluid sample pretreatment technology is main
Have：Liquid-liquid extraction, liquid film extraction, Solid Phase Extraction, purging capture, liquid-phase micro-extraction etc..Wherein liquid-liquid extraction and Solid Phase Extraction
It is main extracting process.
Liquid-liquid extraction（LLE）It is to distribute solubility and distribution in two kinds of unmixing solvents using sample different component
The difference of ratio detaches to reach, the purpose of extraction or purifying, has a wide range of application, technology maturation, processing sample size is larger, extracts
Compare completely.But it is cumbersome, take it is longer, do not have automation, organic solvent consumption is big, extraction when occur emulsify or
Precipitation.The shortcomings that due to liquid-liquid extraction, limits its application；And liquid-liquid sample pre-treatments realize that full automatic treatment is also mainly deposited
In following difficulty：
1. liquid-liquid is sufficiently mixed；
2. liquid-liquid easily emulsifies after being sufficiently mixed；
3. needing to carry out break milk separation with supercentrifuge after emulsification, difficulty is brought to automation using supercentrifuge；
4. after break milk separation forms liquid-liquid layering, the extraction of organic solvent fully relies on human eye and the operation of hand is completed, and requires
There cannot be the ingredient of sample liquid
5. the evaporation after organic solvent extraction is volatilized and generally carried out all in vent cabinet, heated using water-bath, wind is completed
6. being extracted due to the use of organic solvent, test tube, the containers demand used is high, prevents organic solvent from container test tube etc.
Dissolution and the incoherent substance of detection
7. simultaneously because manual operations is difficult to carry out operation related data record
Since there are above-mentioned difficult points, there are no mix from sample, be demulsified, extract organic solvent, up to evaporation volatilizes in the market
Automatic sample processing instrument is still manual operations so far, and error is big, and extraction efficiency is relatively low, and process is cumbersome, and organic solvent is not
The closed progress of energy, environment easy to pollute influence the health of operating personnel so that liquid-liquid extraction is difficult to obtain broader applications.
Invention content
The object of the present invention is to provide a kind of full-automatic liquid-liquid sample treatment instrument, for carrying out pre-treatment to sample, with
Overcome above-mentioned the deficiencies in the prior art.
The technical proposal of the invention is realized in this way, which includes：Solvent delivery system, piece-rate system, purification
With concentration systems, control system, the solvent delivery system is made of solution feeding system and syringe pump system, and the solution supplies
It is attached respectively by main line between system, syringe pump system, purification and concentration systems, piece-rate system, the control
System is electrically connected with solution feeding system, syringe pump system, purification and concentration systems, piece-rate system respectively；
Wherein, the supply for the organic solvent, additive, cleaning agent that the solution feeding system is used for extraction process；
Wherein, the syringe pump system coordinative solvent and is injected into extraction container for quantitatively extracting, and to extraction fluid volume,
Injection pressure, speed and sovent diffusion mode are controlled；
Wherein, the piece-rate system is redistributed for sample and extract liquor mixing, and extract liquor is extracted in demulsification layering；
Wherein, the purification and concentration systems are for removing a small amount of impurity generated in extraction process and moisture and extracting organic
The evaporation of solvent volatilizes；
Wherein, the control system is for extracting Whole Process Control solution feeding system, syringe pump system, piece-rate system, purification
And concentration systems.
Preferably, the solution feeding system includes：At least one container bottle and waste liquid bottle, the container bottle pass through appearance
Device bottle pipeline is connect with solution supply bye-pass, and filter and the second valve, the solution are provided on the container bottle pipeline
It is provided with vacuum purge pump, third valve, the 4th valve and at least one solution supply bye-pass on supply bye-pass and goes out liquid
Mouthful, the third valve and the setting of the 4th valve are in container bottle pipeline both ends, the solution supply bye-pass and vacuum purge pump
Vacuum-pumping pipeline and waste liquid scavenging pipeline are had additional at link position, the vacuum-pumping tube road is provided with vacuum-pumping valve, institute
State waste liquid scavenging pipeline and be provided with waste liquid purging valve, the vacuum-pumping pipeline and waste liquid scavenging pipeline at waste liquid bottle with
Solution supplies bye-pass connection, and the solution supply bye-pass liquid outlet connect with waste liquid bottle, the solution supply bye-pass and
Main line connects, and the main line between the solution feeding system and syringe pump system is equipped with the first valve, the control system
System respectively with filter, vacuum purge pump, the first valve, the second valve, third valve, the 4th valve, vacuum-pumping valve and useless
Liquid purges valve electrical connection.
Preferably, the syringe pump system includes：Pusher, pressure sensor, syringe pump, what the pusher stretched out
The embolism of push rod and syringe pump connects, and the pressure sensor is arranged in push rod, for incude embolism and push rod it
Between extruding force, the injection port of main line and syringe pump between the solution feeding system and syringe pump system passes through syringe pump
Bye-pass is attached, and is also given on the main line between the solution feeding system and syringe pump system useless equipped with syringe pump system
Liquid pipeline is provided with the 5th valve and the 6th valve, the syringe pump system sewer pipe on the main line at the injection port both ends
Road is additionally provided with waste-solution line valve, the control system respectively with pusher, pressure sensor, the 5th valve, the 6th valve
Door and the electrical connection of waste-solution line valve.
Preferably, the piece-rate system includes：Supersonic generator, extraction exchange bottle, breaking emulsion and dewatering device, the extraction
It exchanges bottle to be arranged on supersonic generator, the main line between the syringe pump system and piece-rate system exchanges bottle with extraction and connects
Connect, the extraction exchanges and is provided with nozzle on the main line in bottle, the extraction exchange the extraction that bottle stretches out exchange bye-pass with
Breaking emulsion and dewatering device connects, and the control system exchanges bottle with supersonic generator, extraction respectively, breaking emulsion and dewatering device is electrically connected.
Preferably, the purification and concentration systems include：Evaporation volatilizes bottle, wind turbine, heater, condensing bulb, returnable bottle,
Main line between the piece-rate system and purification and concentration systems volatilizes bottle with evaporation and connect, and the evaporation volatilizes bottle setting and exists
On heater, the evaporation that the evaporation volatilizes bottle stretching volatilizes bye-pass and puts in condensing bulb, the wind turbine from the bottom of bottle of condensing bulb
Escape pipe pass through heater, and escape pipe is heated by heater, the escape pipe volatilizes bottle with evaporation and connect, described
It is connect at the top of the air inlet pipe of wind turbine and condensing bulb, the recovery tube that the condensing bulb stretches out is connect with returnable bottle.
Preferably, the control system includes：Computer, veneer mainboard, control panel and relay board, the calculating
Machine is electrically connected with veneer mainboard, control panel and relay board respectively.
Preferably, being attached by the second air inlet pipe between the returnable bottle and the air inlet pipe of wind turbine, described second
The 7th valve is provided in air inlet pipe.
Preferably, being set respectively on the solution feeding system, syringe pump system, piece-rate system and purification and concentration systems
Set closed guard box.
Preferably, the nozzle be divided into the upper jet blower of upper-spraying type, following spray lower jet blower or pressure jet apparatus,
The upper jet blower is made of the first liquid pipe, the first sap cavity, the first revolving fragment and the first jet blower, the first liquid pipe import with
Extraction exchanges the main line connection in bottle, and first liquid pipe is straight tube-like, and one end and the first liquid pipe of first sap cavity go out
Mouth connection, first revolving fragment are arranged in the first sap cavity, and first jet blower is connect with the other end of the first sap cavity；Institute
Lower jet blower is stated to be made of the second liquid pipe, the second sap cavity, the second revolving fragment and the second jet blower；The second liquid pipe import and extraction
The main line exchanged in bottle is taken to connect, second liquid pipe isType, one end and the outlet of the second liquid pipe of second sap cavity connect
It connects, second revolving fragment is arranged in the second sap cavity, and second jet blower is connect with the other end of the second sap cavity；Mechanical spray
Mouth is exchanged the main line in bottle with extraction and is connected by inlet tube, adjustable speed motor, rotary shaft, jet blower, the inlet tube import,
The inlet tube outlet is connect with jet blower, and the rotary shaft that the adjustable speed motor stretches out is arranged in inlet tube.
Preferably, the pusher includes：Supporting rack, the stepper motor being arranged on supporting rack, stepper motor stretch out
Transmission shaft, the leading screw being connected with transmission shaft, the feed screw nut being arranged on leading screw, push rod is arranged in the feed screw nut.
Advantages of the present invention and good effect are：
1, processing instrument of the invention have it is quick, easy, not only time saving, laborsaving and also can reduce due to different personnel operation and
The error that the multiple transition zone of sample comes, while can be to avoid using a large amount of organic solvents to reduce the pollution to environment.
2, the confession of the valve control progress solution of solution feeding system of the invention gives distribution, opens by setup program,
Respective valves extract different solution, install respective filter additional and ensure that the pure foreign of solution enters instrument, equipped with vacuumizing
Function vacuumizes respective line before solution extraction, ensures that feed flow is smooth, is full of, and is equipped with purging function, can will be not required to
The raffinate wanted is purged to waste liquid bottle, is vacuumized and is purged and is completed by same vacuum purge pump, and it is true to switch pumping using two valves
Empty and purging energy supply.
3, syringe pump system of the invention ensures the precision of syringe pump, and push can be passed through by injecting the speed for being pumped into and promoting
Device with ensure extract exchange process requirement can complete to extract the function of sending out with two tunnels all the way using the control of two valves,
Pressure sensor is arranged in syringe pump, is completely closed in flow observe whether extraction process is normal, and error stops fortune immediately in extraction
Row or alarm.
4, piece-rate system of the invention uses nozzle technology and ultrasonic technology, organic extract liquid in the case where injecting pump pressure
It is sprayed from nozzle, forms organic solvent particle, extraction exchanges bottom of bottle portion and is equipped with ultrasonic generator, using ultrasonic wave organic solvent
It is broken into more small liquid pearl, increases exchange area, ultrasonic wave makes two kinds of liquid that high-frequency vibration be collectively formed, and two kinds of solution are abundant
Contact exchanges, and the short time completes exchange process.
5, purification of the invention and concentration systems use totally-enclosed flow, rear condensing recovery dry to organic solvent hot blow, behaviour
To human body without any contact in work, organic solvent is non-volatile in air, and the organic solvent of recycling can continue to make by reprocessing
With, in addition, evaporation volatilizes bottle, the temperature of wind turbine heater can all set adjustment, it, can for the volatile materials of extraction
The quality that proper temperature reduces the volatilization guarantee extraction of detection substance is adjusted, due to being carried out continuously in closed process, by handing over
The extract liquor changed by into evaporation volatilize bottle, begin to be evaporated the operation volatilized from into fashionable, extraction exchange simultaneously into
Row evaporation volatilizes, and substantially reduces the time of extraction overall process, evaporation volatilizes bottle and conical flask can be used, and low liquid level control is arranged
Device is needing to retain a small amount of extract liquor, when the sample that can be directly detected without constant volume, is reaching specified liquid level, is stopping
Prompt tone is dried up and sent out, evaporation is taken out and volatilizes bottle.
Description of the drawings
Fig. 1 is the overall structure flow chart of the present invention.
Fig. 2 is the syringe pump system overall structure flow chart of the present invention.
Fig. 3 is the solution feeding system overall structure flow chart of the present invention.
Fig. 4 is the piece-rate system syringe pump system overall structure flow chart of the present invention.
Fig. 5 is purification and the concentration systems overall structure flow chart of the present invention.
Fig. 6 is the control system circuit block diagram of the present invention.
Fig. 7 is upper-spraying type nozzle, following spray nozzle and the pressure jet apparatus structural schematic diagram of the present invention.
Fig. 8 is the structural schematic diagram of the pusher of the present invention.
Reference numeral：Solution feeding system A, syringe pump system B, piece-rate system C, purification and concentration systems D, control system
E, main line 1, the first valve 2, container bottle A4, waste liquid bottle A5, container bottle pipeline A6, solution supply bye-pass A7, filter A8,
Second valve A9, it vacuum purge pump A10, third valve A11, the 4th valve A12, solution supply bye-pass liquid outlet A13, takes out
Vacuum line A14, waste liquid scavenging pipeline A15, vacuum-pumping valve A16, waste liquid purging valve A17, pusher B4, pressure sensor
B5, syringe pump B6, push rod B7, embolism B8, injection port B9, syringe pump bye-pass B10, syringe pump system waste-solution line B11,
Five valve B12, the 6th valve B13, waste-solution line valve B14, supporting rack B15, stepper motor B16, leading screw B17, feed screw nut
B18, supersonic generator C4, extraction exchange bottle C5, breaking emulsion and dewatering device C6, nozzle C7, extraction exchange bye-pass C8, upper jet blower
C7-1, the lower jet blower C7-2 of following spray, pressure jet apparatus C7-3, the first liquid pipe C7-1-1, the first sap cavity C7-1-2, the first rotation
Rotor C7-1-3, the first jet blower C7-1-4, the second liquid pipe C7-2-1, the second sap cavity C7-2-1-2, the second revolving fragment C7-2-1-
3, the second jet blower C7-2-4, inlet tube C7-3-1, adjustable speed motor C7-3-2, rotary shaft C7-3-3, jet blower C7-3-4, steaming
Play dry bottle D4, wind turbine D5, heater D6, condensing bulb D7, returnable bottle D8, evaporation volatilize bye-pass D9, escape pipe D10, air inlet
Pipe D11, recovery tube D12, the second air inlet pipe D13, the 7th valve D14, computer E4, veneer mainboard E5, control panel E6 and after
Appliance plate E7.
Specific implementation mode
Refering to fig. 1, the present invention includes：Solvent delivery system, piece-rate system C, purification and concentration systems D, control system E,
The solvent delivery system is made of solution feeding system A and syringe pump system B, the solution feeding system A, syringe pump system
B, be attached respectively by main line 1 between purification and concentration systems D, piece-rate system C, the control system E respectively with it is molten
Liquid supply system A, syringe pump system B, purification and concentration systems D, piece-rate system C electrical connections；The solution feeding system A is used for
The supply of organic solvent, additive, cleaning agent that extraction process uses；The syringe pump system B is corresponding molten for quantitatively extracting
Agent is simultaneously injected into extraction container, and is controlled extraction fluid volume, injection pressure, speed and sovent diffusion mode；It is described
Piece-rate system C is redistributed for sample and extract liquor mixing, and extract liquor is extracted in demulsification layering；The purification and concentration systems D
Evaporation for removing a small amount of impurity generated in extraction process and moisture and extraction organic solvent volatilizes；The control system
E is for extracting Whole Process Control solution feeding system, syringe pump system, piece-rate system and purification and concentration systems；The solution
It is separately provided for solution feeding system on feed system A, syringe pump system B, piece-rate system C, purification and concentration systems D
A, syringe pump system B, piece-rate system C, purification and concentration systems D are in the closed guard box in full-closed environment.
Referring to Fig.2, the solution feeding system A includes：At least one container bottle A4 and waste liquid bottle A5, the container bottle A4
Bye-pass A7 is supplied with solution to connect, filter A8 and second is provided on the container bottle pipeline A6 by container bottle pipeline A6
Vacuum purge pump A10, third valve A11, the 4th valve A12 and extremely are provided on valve A9, the solution supply bye-pass A7
Few solution supply bye-pass liquid outlet A13, the third valve A11 and the 4th valve A12 are arranged in container bottle pipeline A6
Vacuum-pumping pipeline A14 is had additional at both ends, the solution supply bye-pass A7 and vacuum purge pump A10 link positions and waste liquid is blown
Sweeping setting on pipeline A15, the vacuum-pumping pipeline A14, there are two vacuum-pumping valve A16, the waste liquid scavenging pipeline A15 settings
There are two waste liquid purging valve A17, the vacuum-pumping pipeline A14 and waste liquid scavenging pipeline A15 at waste liquid bottle A5 with it is molten
Liquid supplies bye-pass A7 connections, and the solution supply bye-pass liquid outlet A13 is connect with waste liquid bottle A5, and the solution supplies branch pipe
Main line 1 between road A7 and solution feeding system A, syringe pump system B connects, the solution feeding system A and syringe pump system
The main line 1 between B of uniting is equipped with the first valve 2, the control system E respectively with filter A8, vacuum purge pump A10, the
Two valve A9, third valve A11, the 4th valve A12, vacuum-pumping valve A16 and waste liquid purging valve A17 electrical connections.
Refering to Fig. 3 and Fig. 8, the syringe pump system B includes：Pusher B4, pressure sensor B5, syringe pump B6, it is described
The push rod B7 that pusher B4 stretches out is connect with the embolism B8 of syringe pump B6, and the pressure sensor B5 is arranged in push rod B7
On, for incuding the extruding force between embolism B8 and push rod B7, between the solution feeding system A and syringe pump system B
The injection port B9 of main line 1 and syringe pump B6 is attached by syringe pump bye-pass B10, the solution feeding system A and note
It is also given on the main line 1 penetrated between pumping system B equipped with syringe pump system waste-solution line B11, the supervisor at the both ends the injection port B9
The 5th valve B12 and the 6th valve B13, the 5th valve B12 and the 6th valve B13 is provided on road 1 to be arranged in injection port
Near B9, be additionally provided on the syringe pump system waste-solution line B11 waste-solution line valve B14, the control system E respectively with
Pusher B4, pressure sensor B5, the 5th valve B12, the 6th valve B13 and the B14 electrical connections of waste-solution line valve, wherein push away
The device B4 is sent to include：The transmission shaft that supporting rack B15, the stepper motor B16 being arranged on supporting rack B15, stepper motor B16 stretch out,
Push rod is arranged in the leading screw B17 being connected with transmission shaft, the feed screw nut B18, the feed screw nut B18 being arranged on leading screw B17
B7。
Refering to Fig. 4, the piece-rate system C includes：Supersonic generator C4, extraction exchange bottle C5, breaking emulsion and dewatering device C6, institute
It states extraction and exchanges bottle C5 settings on supersonic generator C4, the main line 1 between the syringe pump system B and piece-rate system C
Bottle C5 connections are exchanged with extraction, the extraction, which exchanges, is provided with nozzle C7 on the main line 4 in bottle C5, the extraction exchanges bottle C5
The extraction of stretching exchanges bye-pass C8 and is connect with breaking emulsion and dewatering device C6, the control system E respectively with supersonic generator C4, extract
It takes and exchanges bottle C5, the C6 electrical connections of breaking emulsion and dewatering device.
Refering to Fig. 7, the nozzle C7 point is the upper jet blower C7-1 of upper-spraying type, the lower jet blower C7-2 of following spray or
Pressure jet apparatus C7-3, the upper jet blower C7-1 is by the first liquid pipe C7-1-1, the first sap cavity C7-1-2, the first revolving fragment C7-1-3
With the first jet blower C7-1-4 compositions, the first liquid pipe C7-1-1 imports exchange the main line 4 in bottle C5 with extraction and connect, institute
It is straight tube-like to state the first liquid pipe C7-1-1, and one end of the first sap cavity C7-1-2 is connected with the first outlets liquid pipe C7-1-1, institute
It states the first revolving fragment C7-1-3 to be arranged in the first sap cavity C7-1-2, the first jet blower C7-1-4 and the first sap cavity C7-1-2
The other end connection；The lower jet blower C7-2 is by the second liquid pipe C7-2-1, the second sap cavity C7-2-1-2, the second revolving fragment C7-
2-1-3 and the second jet blower C7-2-4 compositions；The second liquid pipe C7-2-1 imports exchange the main line 4 in bottle C5 with extraction and connect
It connects, the second liquid pipe C7-2-1 isType, one end of the second sap cavity C7-2-1-2 connect with the second outlets liquid pipe C7-2-1
It connects, the second revolving fragment C7-2-1-3 is arranged in the second sap cavity C7-2-1-2, the second jet blower C7-2-4 and second
The other end of sap cavity C7-2-1-2 connects；Pressure jet apparatus C7-3 is by inlet tube C7-3-1, adjustable speed motor C7-3-2, rotary shaft
C7-3-3, jet blower C7-3-4, the inlet tube C7-3-1 imports with extraction exchanges in bottle C5 main line 4 connection, it is described into
The outlets liquid pipe C7-3-1 are connect with jet blower C7-3-4, and the rotary shaft C7-3-3 that the adjustable speed motor C7-3-2 stretches out is set
It sets in inlet tube C7-3-1.
The supersonic generator C4 includes：Intensity controlled supersonic generator plate and ultrasonic converter.
Piece-rate system C major functions are to ensure the abundant exchange process of sample and organic solvent, minimum to emulsify, is minimum
It is aqueous（In sample）, to greatest extent extract extract liquor with ensure extraction efficiency and accuracy, while again do not use high speed from
Heart method is convenient for automation mechanized operation.Piece-rate system C features are as follows：Use totally-enclosed, continuous liquid-liquid extraction pattern；Using
Nozzle technology and ultrasonic technology spray organic extract liquid from nozzle C7 under syringe pump B6 pressure, it is micro- to form organic solvent
Grain, extraction exchange the bottoms bottle C5 and are equipped with ultrasonic generator C4, and organic solvent is broken into more small liquid pearl using ultrasonic wave, increase
Exchange area, ultrasonic wave make two kinds of liquid that high-frequency vibration be collectively formed, and two kinds of solution come into full contact with exchange, and the short time completes to hand over
Change process；Entire exchange process is completed by being demulsified, absorbing water.
Organic solvent is continuously advanced to extraction and exchanges bottle C5 by syringe pump B6, is sprayed by nozzle C7, and organic solvent is formed
Fine droplet, fine droplet flow through sample solution and swap, and organic solvent passes through after sample solution top reaches predetermined amount
Connecting tube enters evaporation and volatilizes a bottle D4.Since extraction process is to be carried out continuously, recovery of extraction is primary higher than the prior art
Property hybrid extraction.The formula that two solutions of liquid-liquid extraction exchanges distribution is as follows：
（For distribution constant）
Disposable mixed allocation extraction, extraction results are in this way：
,：Extraction factor,=N.D → distribution coefficient, N：Compared to=
Row is total to single extraction organic solvent 8ml, and 80%,
In same volume accumulated amount, organic solvent is divided into four 1. 3ml, 2. 2ml, 3. 2ml 4. 1ml（Identical organic solvent
Amount）Hybrid extraction, result are as follows：
It is extracted it can be seen that the result for being divided into four extractions is better than primary mix, extraction by hand often divides to obtain better effects
It is carried out at secondary to four times, operating process is more complicated, and the time is elongated, and the application is due to being carried out continuously extraction, into sample
Organic solvent is to start from scratch, and is floated after exchange（Decline）It rolls up a certain amount of entrance and volatilizes bottle, control and retain organic solvent
Amount, can be improved recovery of extraction, is equivalent to the integral of formula point n times, effect of extracting reaches best.
To improve extraction efficiency, refinement organic solvent fluid pearl, increasing mixing intensity in this case can stages of labor degree difference
Emulsification, can be solved under high speed centrifugation, although this instrument takes nozzle and ultrasonic technique to substantially reduce emulsification, slight breast
Change also will produce, and for slightly emulsifying be handled using demulsification plus water suction pattern.Emulsification is two kinds of situations；1 is that sample is small
Drop wraps organic solvent drop and forms emulsification；2 be organic solvent drop package sample drop
Since the emulsification of this instrument is mainly the first situation, it is demulsified using demulsification column and water suction.Use patent（ZL 2013
2 0294270.9）Dominant mechanism：
It will produce when by mutually insulated different metal foam synusia 1. sample solution is mainly the aqueous solution to contain salt
Weak current makes to be wrapped in the disengaging of organic solution drop free surface moisture；
2. having electret covering layer outside demulsification column, there is high electrostatic field negative potential, passes through in the liquid by extraction microemulsified
When, the sample hydrone of package organic solvent drop can be stripped under negative potential effect
3. demulsification column entrance has filtering plug, filtering, which is plugged with, can select micro-pore, and the solution after extraction passes through micro-pore
When also play the role of demulsification；
4. being separated by demulsification column demulsification organic solvent and sample aqueous solution, pass through water absorbing agent（Only organic solvent is not inhaled in water suction）Make
Water stays in water absorbing agent,
The exchange process of entire liquid-liquid extraction is completed by the water suction that is demulsified above.
Refer to patent（ZL 2013 2 0294270.9）.
It since the volatilization temperature of organic solvent is less than water, volatilizees quickly, can be taken away in volatilization a large amount of at moderate temperatures
Heat, and water is almost non-volatile at such temperature, there is sample（Water）On the one hand the impurity of extraction can be made to increase into volatilizer, together
Shi great great delays the speed of volatilization.By being demulsified, water suction can solve sample substantially（Water）Into volatilization container, volatilization speed is improved
Spend and reduce extracting impurities.Using the treating method of demulsification column demulsification and dehydration, avoided using breaking emulsion and dewatering is completed by formula
High speed centrifugation carries out breaking emulsion and dewatering, makes instrument automation easy to implement.
Refering to Fig. 5, the purification and concentration systems D include：Evaporation volatilizes a bottle D4, wind turbine D5, two heater D6, condensation
Bottle D7, returnable bottle D8, the main line 1 between the piece-rate system C and purification and concentration systems D volatilize a bottle D4 with evaporation and connect,
The evaporation volatilizes bottle D4 and is arranged on heater D6, and the evaporation volatilizes the evaporation that bottle D4 stretches out and volatilizes bye-pass D9 from condensation
The escape pipe D10 that the bottom of bottle of bottle D7 puts in condensing bulb D7, the wind turbine D5 passes through heater D6, and by heater D6 to escape pipe
D10 is heated, and the escape pipe D10 volatilizes a bottle D4 with evaporation and connect, and the air inlet pipe D11 and condensing bulb D7 of the wind turbine D5 are pushed up
Portion connects, and the recovery tube D12 that the condensing bulb D7 stretches out connect D8, the air inlet pipe of the returnable bottle D8 and wind turbine D5 with returnable bottle
It is attached by the second air inlet pipe D13 between D11, the 7th valve D14, the steaming is provided on the second air inlet pipe D13
It is conical flask to play dry bottle D4, and the conical flask is provided with low liquid level controller.
Refering to Fig. 6, the control system E includes：Computer E4, veneer mainboard E5, control panel E6 and relay board E7,
The computer E4 is electrically connected with veneer mainboard E5, control panel E6 and relay board E7 respectively.
The course of work：
1, it extracts respective sample and is put into extraction exchange bottle C5, be put into breaking emulsion and dewatering device C6, evaporation volatilizes a bottle D4, connects respective tube
Road.
2, start syringe pump system B and solution feeding system A, extract corresponding solution injection extraction and exchange bottle C5, You Jirong
Agent forms fine droplet at nozzle C7 and ultrasonic wave collective effect and completes to exchange assigning process by sample.
3, organic solvent completes exchange process, and breaking emulsion and dewatering device C6 is initially entered after reaching default constant volume, completes broken
Evaporation, which is automatically flowed into, after the de- sample liquid of breast volatilizes bottle,
4, the solvent that bottle D4 is volatilized into evaporation is heated, and hot-air blowing volatilization, organic solvent gas enters condensation after volatilization
Bottle D7 carries out condensing recovery
5, it is drawn according to set amount syringe pump B6 and accordingly quantifies pure water or air, extraction organic solvent imported completely evaporation and waved
It is volatilized in dry bottle D4, completes all extractions
6, it after completion evaporation volatilizes, takes out evaporation and volatilizes a bottle D4, carry out constant volume, for detecting instrument use.
Claims (10)
1. full-automatic liquid-liquid sample treatment instrument, which is characterized in that including：Solvent delivery system, piece-rate system, purification and concentration
System, control system, the solvent delivery system are made of solution feeding system and syringe pump system, solution supply system
It is attached respectively by main line between system, syringe pump system, purification and concentration systems, piece-rate system, the control system
It is electrically connected respectively with solution feeding system, syringe pump system, purification and concentration systems, piece-rate system；
Wherein, the supply for the organic solvent, additive, cleaning agent that the solution feeding system is used for extraction process；
Wherein, the syringe pump system coordinative solvent and is injected into extraction container for quantitatively extracting, and to extraction fluid volume,
Injection pressure, speed and sovent diffusion mode are controlled；
Wherein, the piece-rate system is redistributed for sample and extract liquor mixing, and extract liquor is extracted in demulsification layering；
Wherein, the purification and concentration systems are for removing a small amount of impurity generated in extraction process and moisture and extracting organic
The evaporation of solvent volatilizes；
Wherein, the control system is for extracting Whole Process Control solution feeding system, syringe pump system, piece-rate system, purification
And concentration systems.
2. full-automatic liquid-liquid sample treatment instrument according to claim 1, which is characterized in that the solution feeding system packet
It includes：At least one container bottle and waste liquid bottle, the container bottle supply bye-pass with solution by container bottle pipeline and connect, the appearance
It is provided with filter and the second valve on device bottle pipeline, vacuum purge pump, third valve are provided on the solution supply bye-pass
Door, the 4th valve and at least one solution supply bye-pass liquid outlet, and the third valve and the 4th valve are arranged in container bottle
Pipeline both ends, the solution supply and have additional vacuum-pumping pipeline and waste liquid scavenging conduit at bye-pass and vacuum purge pump link position
Road, the vacuum-pumping tube road are provided with vacuum-pumping valve, and the waste liquid scavenging pipeline is provided with waste liquid purging valve, the pumping
Vacuum line and waste liquid scavenging pipeline are being connect at waste liquid bottle with solution supply bye-pass, and the solution supply bye-pass goes out
Liquid mouth is connect with waste liquid bottle, and the solution supply bye-pass is connect with main line, the solution feeding system and syringe pump system
Between main line be equipped with the first valve, the control system respectively with filter, vacuum purge pump, the first valve, second
Valve, third valve, the 4th valve, vacuum-pumping valve and waste liquid purging valve electrical connection.
3. full-automatic liquid-liquid sample treatment instrument according to claim 1, which is characterized in that the syringe pump system includes：
The embolism of pusher, pressure sensor, syringe pump, push rod and syringe pump that the pusher stretches out connects, and the pressure passes
Sensor is arranged in push rod, for incuding the extruding force between embolism and push rod, the solution feeding system and syringe pump
The injection port of main line and syringe pump between system is attached by syringe pump bye-pass, the solution feeding system and note
It is also given on the main line penetrated between pumping system equipped with syringe pump system waste-solution line, is arranged on the main line at the injection port both ends
There are the 5th valve and the 6th valve, waste-solution line valve, the control system are additionally provided on the syringe pump system waste-solution line
System is electrically connected with pusher, pressure sensor, the 5th valve, the 6th valve and waste-solution line valve respectively.
4. full-automatic liquid-liquid sample treatment instrument according to claim 1, which is characterized in that the piece-rate system includes：It is super
Sonic generator, extraction exchange bottle, breaking emulsion and dewatering device, and the extraction exchanges bottle and is arranged on supersonic generator, the injection
Main line between pumping system and piece-rate system exchanges bottle connection with extraction, and the extraction exchanges to be provided on the main line in bottle
Nozzle, it is described extraction exchange bottle stretch out extraction exchange bye-pass connect with breaking emulsion and dewatering device, the control system respectively with surpass
Sonic generator, extraction exchange bottle, the electrical connection of breaking emulsion and dewatering device.
5. full-automatic liquid-liquid sample treatment instrument according to claim 1, which is characterized in that the purification and concentration systems
Including：Evaporation volatilizes bottle, wind turbine, heater, condensing bulb, returnable bottle, between the piece-rate system and purification and concentration systems
Main line volatilizes bottle with evaporation and connect, and the evaporation volatilizes bottle setting on the heaters, and the evaporation volatilizes the evaporation of bottle stretching
It volatilizes bye-pass and puts in condensing bulb from the bottom of bottle of condensing bulb, the escape pipe of the wind turbine passes through heater and by heater to going out
Tracheae is heated, and the escape pipe volatilizes bottle with evaporation and connect, and is connect at the top of the air inlet pipe and condensing bulb of the wind turbine, described
The recovery tube that condensing bulb stretches out is connect with returnable bottle.
6. full-automatic liquid-liquid sample treatment instrument according to claim 1, which is characterized in that the control system includes：Meter
Calculation machine, veneer mainboard, control panel and relay board, the computer respectively with veneer mainboard, control panel and relay board
Electrical connection.
7. full-automatic liquid-liquid sample treatment instrument according to claim 5, it is characterised in that：The returnable bottle and wind turbine
It is attached by the second air inlet pipe between air inlet pipe, the 7th valve is provided in second air inlet pipe.
8. full-automatic liquid-liquid sample treatment instrument according to claim 1, it is characterised in that：The solution feeding system, note
It penetrates on pumping system, piece-rate system and purification and concentration systems and closed guard box is respectively set.
9. full-automatic liquid-liquid sample treatment instrument according to claim 4, it is characterised in that：The nozzle is divided into upper-spraying type
The lower jet blower or pressure jet apparatus of upper jet blower, following spray, the upper jet blower is by the first liquid pipe, the first sap cavity,
One revolving fragment and the first jet blower composition, the first liquid pipe import exchange the main line in bottle with extraction and connect, and described first
Liquid pipe is straight tube-like, and one end and the outlet of the first liquid pipe of first sap cavity connect, and first revolving fragment is arranged in the first liquid
Intracavitary, first jet blower are connect with the other end of the first sap cavity；The lower jet blower is by the second liquid pipe, the second sap cavity,
Two revolving fragments and the second jet blower composition；The second liquid pipe import exchanges the main line in bottle with extraction and connects, and described second
Liquid pipe isType, one end and the outlet of the second liquid pipe of second sap cavity connect, and second revolving fragment is arranged in the second sap cavity
Interior, second jet blower is connect with the other end of the second sap cavity；Pressure jet apparatus is by inlet tube, adjustable speed motor, rotary shaft, spray
Nozzle, the inlet tube import exchange the main line in bottle with extraction and connect, and the inlet tube outlet is connect with jet blower, described
The rotary shaft that adjustable speed motor stretches out is arranged in inlet tube.
10. full-automatic liquid-liquid sample treatment instrument according to claim 3, it is characterised in that：The pusher includes：Branch
The transmission shaft that support, the stepper motor being arranged on supporting rack, stepper motor stretch out, the leading screw being connected with transmission shaft, setting exist
Push rod is arranged in feed screw nut on leading screw, the feed screw nut.
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